Orthovanadic-acid esters and their solutions.



Per

LUnWie-nnss', vor sentimenten. Gamarra.

No Drawing.

T0 all w/iom it may concern:

Be it known that I, Dr. Lnowrs i-lues, a subject of the German Emperor, residing at Berlin-Britz, Germany, have invented 'certain new and useful Improvements Relating to OrthoVanadic-Acid Esters and Their Solutions, of which the following is a specication.

I have found that, contrary to the hither-z to existing statements in the literature, va

nadium pentoxid dissolves in the most varied 'pr1mary, secondary and tertiary monoand polyhydric alcohols With the forma-tion of esters, and that from the solutions in the primary, secondary and tertiary alcohols esters 'of the constitution RSVO, (Rzradical) can be isolated which are either liquid orsolid, colored or colorless according to the nature of the alcohol employed.k

The process for producing such esters or ester solutions is as follows luPm'mm'y alcohols-Ethyl alcohol for example is boiled `with an excess of vanadium pentoxid for several hours under areluX condenser, the excess of alcohol driven oil` and the ester which remains behind distilled over como. lts formula is The ester is a slightly colored liquid,which atv15 C. has a density of 1.167. At 26 mm. pressure its boiling point is 108.0 C.

Il. Seconda/ry' alcoholsfwlsopropyl alcohol for example is boiled with an excess of a reflugrcondenser. The almost colorless solution is then subjected to fractional distil lation in vacuo, a colorless ester being obtained whichaccording'to analysis and determination of its molecular weight has the formula @Horrorlte specic gravity at 15 C. is 0.993, and

application and retinal-gf e, wie. 'sentirne atraso.

.onrncvnimnic-ncmnsrnns 'main sorurion's 'Specification ot Letters etent. 'l Palmg gag, 3

'its boilingpoiiit at pressure of 19 161 C. When heated in the open air the ester gradually becomes colored light Igreen and at about 206 it boils with decomposiu tion. lt dissolves easily in alcohol, ether, benzol, toluol, chloroform and acetone 'and on prolonged boiling with water is decom-v posed with the formation of amylene hy drate and the separation of ranadic acid.

IV. lf glycerin, glycol or benzyl alcohol be heated with V205, solutions of e slight yellow color are obtained which contain more or lessvanadium in ester form.

The products obtained 'are intended for use for pharmaceutical purposes or as valuable raw materials.

It should be pointed out that except the two following points nothing" has been known hitherto about obtaining vanadic acid esters. K

1. YV. Prandtl publishes a statement i the Handbuch der inorganica/Len Chemie by GmeZz'nJfmut, VH edition, lll Vol. pages 86 and 91 on lhe obtaining of an extremely unstable vanadic acid ethyl ester and its ethyl alcoholic solution of the composition V,`05.C2H5OH.H20,

and which he obtains by treating a melt of vanadium pentoxid' and boricacid withal cohol. This statement does notV concer-xl this invention, as it is not known to convert V205 directly into esters by boiling 'with alcohol,

and also no ester of the constitution RSVO,

was obtained.'4 The new esters diii'er also from the known products in mostvcases by their unlimited stability.

2. Hall (Journal Chem. Soc. London 51, 1887, page 751) has prepared small quantities of orthovanadic acid ester from silver orthovanadates and halogen alkyls.

1. The process for the manufacture of ortho-vanadic acid esters, which consists in boiling an alcohol with vanadium pentoxid, substantially as described.

2. The process for the manufacture of ortho-vanadic acid esters, ywhich consists in boiling an alcohol with vanadium pentoxld and separating the ester thus reduced from distillation,

the product of the reaction, y substantially as described.

A colorless liquid having at 157C. (le

, 3.v lThe process for the manufacture of tei'- tiary amyl-esters of ortho-vanadic4 acid,

'which 4consists in boiling amylenehydrate with ygnaidium pentoxid under reux con- 5 .denser, and 'se arating 'theesteij from the a solution thus o tained, by fractional distilon n o acuo, substantially as described.

As a new product,'the tertiary'amyliaspeciclgpgvzity of 0.993, boiling at l1610A C. Lynde@ Pres/Sue :0f ,19 mns-, gradually .as-

geen.: eeleufuhepyheatd in the air to 1009 C., boiling at about 206 C.,

lrating out Vanadic a cid,substantial1y as described.

` In testimony whereof I `'have hereunto set my hand iny presence of two subscribing witnesses. 1 l

DR. LUDWIGJESS. f

l Witnesses: r

t. MARC FUCHS,

RUDOLF ,GERER 

